US10870947B2 - Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors - Google Patents

Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors Download PDF

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US10870947B2
US10870947B2 US16/326,769 US201716326769A US10870947B2 US 10870947 B2 US10870947 B2 US 10870947B2 US 201716326769 A US201716326769 A US 201716326769A US 10870947 B2 US10870947 B2 US 10870947B2
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hemicelluloses
stream
range
suspended solids
incoming stream
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US20190203416A1 (en
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Oleg Shagaev
Lukas Wiesegger
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Andritz AG
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Andritz AG
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0007—Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0042—Fractionating or concentration of spent liquors by special methods
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0085—Introduction of auxiliary substances into the regenerating system in order to improve the performance of certain steps of the latter, the presence of these substances being confined to the regeneration cycle
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/04—Regeneration of pulp liquors or effluent waste waters of alkali lye
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/10—Concentrating spent liquor by evaporation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • Disclosed herein is a process for isolation of hemicelluloses from biomass pulping process waters and spent liquors with removal of suspended solids, concentration of the product and purification of the product by removal of inorganic salts and low molecular weight substances.
  • a hemicellulose isolation process conditions at several separation/purification stages are adjusted separately by pH adjustment, where the pH value of the clear fluid stream after removal of coarse suspended solids is adjusted to pH 8-11, preferably pH 9.0-9.5, whereby the pH value of the incoming effluent stream is adjusted to pH 8-11 and before removal of inorganic salts the pH value is adjusted to 4.0-4.5.
  • the final product enriched with hemicellulose after separation of ashes has a dryness of 15-30%. This allows cheaper thermal isolation treatment afterwards.
  • FIG. 1 shows the typical setup of the preferred process.
  • This process for isolation of hemicelluloses can be used for mechanical pulping lines, semi-chemical and chemical pulping plants. It can be implemented in either existing installations or rebuild projects.
  • the process applies for biomass, hardwood (xylans) and softwoods (galactoglucomannans (GGM)) pulping lines process waters and spent liquors treatment where alkaline treatment or high temperature water extraction of biomass is used.
  • Typical pulping lines for isolation of hemicelluloses from process waters, bleach plants and spent liquors are:
  • the incoming stream A in FIG. 1 can be any effluent of any mechanical or semi-chemical pulping line containing hemicellulose, which can be e.g. white water or pressate, or filtrate, or black liquor from pulp washing equipment normally at a temperature of e.g. 60-90° C.
  • the incoming stream A loaded with a high amount of COD (chemical oxygen demand) as “effluent” is usually sent to an effluent treatment station, which is the current state-of-the-art.
  • COD chemical oxygen demand
  • the pH is adjusted to pH 8-11 by stream B.
  • stream C containing coarse suspended solids, such as fibers and fiber particles and particles greater than >10 ⁇ m that are not retained during washing are removed in the first process step I, whereby some separation equipment allows to remove particles greater than >5 ⁇ m.
  • Process step I can be performed by mechanical separation equipment such as filtration units or centrifuges (e.g. decanter centrifuge).
  • a decanter centrifuge e.g. decanter centrifuge
  • the necessity to use for example a decanter centrifuge is suitable for the APMP lines without existing fiber recovery system (e.g. fiber recovery disc filter) that is capable to remove fiber fragments, fines and other suspended solids from screw press pressate after an alkaline peroxide bleaching stage.
  • the decanter centrifuge is used to remove suspended solids.
  • existing fiber recovery system e.g. having the fiber recovery disc filter
  • pulp washing equipment e.g. screw pressate after alkaline peroxide bleaching stage
  • the usage of decanter centrifuge is optional, or can be eliminated.
  • adjustment of the pH value may only be done with adding the basic chemicals in stream B, in other applications chemical addition to get to pH 8-11, preferably 9.0-9.5, can be done in stream H.
  • this fraction is transferred to the liquid phase of the effluent—stream G′—and is sent to process step II, where smaller particles in the range of >0.5-10 ⁇ m are removed, e.g. very fine biomass material and colloidal suspended solids (e.g. silicates, resins).
  • colloidal suspended solids e.g. silicates, resins
  • machines and equipment such as centrifugal disc separators (or other type of separators), or membrane type micro filtration units can be used.
  • the effluent J is sent to process step III, in which the hemicelluloses are enriched.
  • reject streams of process step I—stream D—and of process step II—stream E, containing fibers and other suspended solids down to approx. 0.5 ⁇ m particle size, are collected and can be sent back to the system (mechanical or semi-chemical pulping line or pulp and paper mill)—stream F.
  • process step III usually ultrafiltration membrane units are used and most of the water, salts and low molecular organics are removed and the effluent/product is concentrated to a factor of 10-20.
  • stream K having much less COD (chemical oxygen demand) than stream A thus can be reused in the system (mechanical or semi-chemical pulping line or pulp and paper mill).
  • the pH of the concentrated liquor/effluent L is adjusted by stream M and the resulting stream N is passed through to the next process step IV, which is a membrane unit—usually diafiltration, where stream N is washed by fresh water or process condensate—stream P and inorganic salts (mostly sodium) are removed to the required product quality level and the product is concentrated further to the level of solids content sufficient for the next process step(s).
  • the pH of stream L is adjusted to pH 4.0-4.5 by acid, e.g. sulfuric acid, hydrochloric acid etc. by stream M in order to have more efficient removal of bound sodium ions (Na + ) and, correspondingly, reduce the product ash content further if required.
  • Process step IV is able to produce the product (stream Q) at 20-30% solids concentration.
  • Process step IV generates excess water/permeate O, which can be used for dilution or any further use in the system (mechanical or semi-chemical pulping line or pulp and paper mill) to substitute fresh water or any mill water.
  • the out coming stream Q of process step IV is further processed in process step V, where the hemicelluloses are thickened further up to a solid concentration of 50-80%.
  • Process step (V) can usually be a thermal separation process such as evaporation, which generates excess water of high quality, typically condensate, —stream R, which can be used for the diafiltration stage (step IV), dilution or any further use in the system (mechanical or semi-chemical pulping line or pulp and paper mill) to substitute fresh water or any mill water.
  • the heating of the thermal drying unit may be achieved by waste steam from the mill.
  • the out coming stream S of process step V can be used as a product or depending on the final product concentration requirements (e.g. 80-90% dry solids) is thickened further in another process step VI, which can be a drying unit, e.g. spray dryer.
  • the final product enriched with hemicellulose encompasses a dryness level of 50-80% as slurry/suspension, paste or gel—stream S or if necessary around 80-90% as powder—stream T.
  • the invention is not limited to the drawing but the process may also already end after process step IV when the stream may be further used in the system. Also excess water (stream R) of process step V may be reused instead of fresh water for stream P of process step IV.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Sustainable Development (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Molecular Biology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Paper (AREA)
  • Processing Of Solid Wastes (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
US16/326,769 2016-09-02 2017-07-27 Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors Active 2037-09-29 US10870947B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
ATA50780/2016A AT519059B1 (de) 2016-09-02 2016-09-02 Verfahren zur Abtrennung von Hemizellulosen aus Biomasse-Aufschlussprozesswasser oder verbrauchten Laugen
ATA50780/2016 2016-09-02
PCT/EP2017/069032 WO2018041488A1 (en) 2016-09-02 2017-07-27 Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors

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US20190203416A1 US20190203416A1 (en) 2019-07-04
US10870947B2 true US10870947B2 (en) 2020-12-22

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US (1) US10870947B2 (de)
EP (1) EP3507415B1 (de)
JP (1) JP6752359B2 (de)
CN (1) CN109642394B (de)
AT (1) AT519059B1 (de)
AU (1) AU2017318207B2 (de)
BR (1) BR112019001781B1 (de)
CA (1) CA3035614C (de)
CL (1) CL2019000545A1 (de)
RU (1) RU2713239C1 (de)
WO (1) WO2018041488A1 (de)

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CN111961695B (zh) * 2020-07-02 2022-07-29 上海昶法新材料有限公司 利用溶解浆预蒸煮废液制备低聚糖的方法
CN111943994B (zh) * 2020-07-02 2022-02-01 上海昶法新材料有限公司 利用溶解浆预蒸煮废液制备木糖的方法

Citations (8)

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US4470876A (en) 1982-07-22 1984-09-11 Beaupre Marc F Kraft overload recovery process
WO2002040767A1 (en) 2000-11-16 2002-05-23 Raisio Chemicals Ltd Method for recovering non-fibrous substances from wood material
WO2004013409A1 (en) 2002-07-25 2004-02-12 Coffin World Water Systems Apparatus and method for treating black liquor
US20120196233A1 (en) 2011-02-01 2012-08-02 Yonghao Ni Recovery of dissolved organics from lignocellulosic solutions
US20130115653A1 (en) * 2011-11-09 2013-05-09 Thesis Chemistry, Llc Method for producing biobased chemicals from woody biomass
US20140163245A1 (en) 2011-05-26 2014-06-12 Michael A. Lake Process for producing furfural from black liquor
US20170215471A1 (en) * 2016-02-02 2017-08-03 R.J. Reynolds Tobacco Company Method for preparing flavorful compounds isolated from black liquor and products incorporating the flavorful compounds
US20190249363A1 (en) * 2016-10-11 2019-08-15 Clariant International Ltd. Method for extracting cellusose, hemicellulose and lignin from lignocellulose from plant biomass

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AT413697B (de) * 2001-11-07 2006-05-15 Andritz Ag Maschf Verfahren zur behandlung säurehältiger abwässer
US7101996B2 (en) * 2003-09-23 2006-09-05 Corn Products International, Inc. Process for preparing purified fractions of hemicellulose and cellulose-hemicellulose complexes from alkali treated fiber and products made by the process
FI120045B (fi) * 2005-12-22 2009-06-15 Roal Oy Selluloosamateriaalin käsittely ja siinä käyttökelpoiset entsyymit
JP2011019489A (ja) * 2009-07-21 2011-02-03 Hbi Kk 水溶性ヘミセルロースの調製方法
CN102838693A (zh) * 2011-06-21 2012-12-26 北京林业大学 从生物质中分离纯化直链半纤维素和支链半纤维素的方法
US20160130752A1 (en) * 2013-05-29 2016-05-12 Kiram Ab Method for the treatment of spent pulping liquor for the removal and production of a lignin containing product
CN103541260A (zh) * 2013-10-28 2014-01-29 宜宾海丝特纤维有限责任公司 一种从制浆黑液中回收半纤维素的方法
WO2016033456A1 (en) * 2014-08-29 2016-03-03 University Of Tennessee Research Foundation Comprehensive process for selectively separating lignocellulosic biomass into purified components with high yield
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Publication number Priority date Publication date Assignee Title
US4470876A (en) 1982-07-22 1984-09-11 Beaupre Marc F Kraft overload recovery process
WO2002040767A1 (en) 2000-11-16 2002-05-23 Raisio Chemicals Ltd Method for recovering non-fibrous substances from wood material
WO2004013409A1 (en) 2002-07-25 2004-02-12 Coffin World Water Systems Apparatus and method for treating black liquor
US20120196233A1 (en) 2011-02-01 2012-08-02 Yonghao Ni Recovery of dissolved organics from lignocellulosic solutions
US20140163245A1 (en) 2011-05-26 2014-06-12 Michael A. Lake Process for producing furfural from black liquor
US20130115653A1 (en) * 2011-11-09 2013-05-09 Thesis Chemistry, Llc Method for producing biobased chemicals from woody biomass
US20170215471A1 (en) * 2016-02-02 2017-08-03 R.J. Reynolds Tobacco Company Method for preparing flavorful compounds isolated from black liquor and products incorporating the flavorful compounds
US20190249363A1 (en) * 2016-10-11 2019-08-15 Clariant International Ltd. Method for extracting cellusose, hemicellulose and lignin from lignocellulose from plant biomass

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Also Published As

Publication number Publication date
AT519059A1 (de) 2018-03-15
EP3507415A1 (de) 2019-07-10
AU2017318207B2 (en) 2021-07-08
CL2019000545A1 (es) 2019-05-31
CA3035614A1 (en) 2018-03-08
WO2018041488A1 (en) 2018-03-08
AU2017318207A1 (en) 2019-02-07
JP2019529612A (ja) 2019-10-17
JP6752359B2 (ja) 2020-09-09
BR112019001781A2 (pt) 2019-05-07
NZ750018A (en) 2024-08-30
AT519059B1 (de) 2018-07-15
US20190203416A1 (en) 2019-07-04
BR112019001781B1 (pt) 2023-04-11
EP3507415B1 (de) 2020-04-01
CA3035614C (en) 2023-05-16
CN109642394B (zh) 2021-07-30
RU2713239C1 (ru) 2020-02-04
CN109642394A (zh) 2019-04-16

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